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Ultrasensitive determination of mercury in waters via photochemical vapor deposition onto quartz substrates coated with palladium nanoparticles followed by total reflection X-ray fluorescence analysis

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Abstract

We describe a method for ultrasensitive detection of mercury (Hg) by total reflection X-ray fluorescence following photogeneration of Hg vapor and trapping onto quartz substrates coated with nanostructured palladium. The nanostructured coating was characterized by transmission electron microscopy. Hg vapor was generated by online photo-UV reduction in the presence of acetic acid, which acts as a precursor for reducing species. Trapping of Hg occurred as a result of amalgamation. A trapping time of 30 min and an acetic acid concentration of 2 mol L−1 provided the best results. An enrichment factor of 127 and a limit of detection as low as 54 ng L−1 of Hg were achieved. The repeatability of the method (expressed as the relative standard deviation at a level of 1 μg L−1) was 3 %. The method was successfully applied to the determination of Hg in water samples spiked with 10 μg L−1 of Hg. Recoveries ranged from 96 to 101 %.

A new method is described for ultrasensitive detection of Hg in natural waters by total reflection X-ray fluorescence following on-line photo UV vapor generation and trapping onto quartz substrates coated with palladium nanoparticles.

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Acknowledgments

The Spanish Ministry of Economy and Competitiveness (Project CTQ2012-32788) and the European Commission (FEDER) is gratefully acknowledged. The Spanish Ministry of Education, Culture and Sport is acknowledged for financial support through a FPU predoctoral grant to V. Romero.

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Authors and Affiliations

  1. Departamento de Química Analítica y Alimentaria, Área de Química Analítica, Facultad de Química, Universidad de Vigo, Campus As Lagoas-Marcosende s/n, 36310, Vigo, Spain

    Vanesa Romero, Inmaculada De La Calle, Isela Lavilla & Carlos Bendicho

  2. Department of Analytical Chemistry, Faculty of Chemistry, Maria Skłodowska-Curie University, Wydział Chemii UMCS w Lublinie pl. M. Curie-Skłodowskiej 2, 20-031, Lublin, Poland

    Magdalena Gryglicka

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  1. Vanesa Romero
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  2. Magdalena Gryglicka
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  3. Inmaculada De La Calle
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  4. Isela Lavilla
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  5. Carlos Bendicho
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Correspondence to Carlos Bendicho.

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Romero, V., Gryglicka, M., De La Calle, I. et al. Ultrasensitive determination of mercury in waters via photochemical vapor deposition onto quartz substrates coated with palladium nanoparticles followed by total reflection X-ray fluorescence analysis. Microchim Acta 183, 141–148 (2016). https://doi.org/10.1007/s00604-015-1612-7

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  • DOI: https://doi.org/10.1007/s00604-015-1612-7

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